A kind of high glow-wire ignition temperature flame-retardant enhanced PBT material and preparation method thereofTechnical field
The present invention relates to technical field of polymer materials, be specifically related to a kind of high glow-wire ignition temperature flame-retardant enhanced PBT material and preparation method thereof.
Background technology
Polybutylene terephthalate (PBT) is a kind of crystallization, line style saturated polyester.It has the features such as excellent mechanical property, electric property, resistance to chemical attack, easy-formation and rate of moisture absorption are low, it is a kind of thermoplastic engineering plastic of high comprehensive performance, be widely used in automobile, electronic apparatus production, part of the part of having relatively high expectations for the manufacture of mechanical strength and heat-resisting, shock-resistant, wear-resisting wiping etc., has become important a member in five large-engineering plastics.Yet, the shortcoming such as pure PBT resin also exists flame retardant resistance bad (can only reach UL-94HB level), physical strength is not high, notched Izod impact strength is low, heat-drawn wire is not high, thus limit it in the application in some field.Therefore at present, in PBT, approximately have 80% to be kind through modification, and the overwhelming majority is flame-retardant enhanced PBT material.Require at present flame-retardant reinforced PBT to pass through the requirement of the IEC60695 of European Union standard more and more general, although there is part producer can reach the requirement of extinguishing in 750 ℃, 2 seconds, but progressively general along with what require, client is more and more harsher to the requirement of extinguishing in these 750 ℃, 2 seconds, general all higher than the temperature of 750 ℃, as required, in 780 ℃, 2 seconds, extinguished, and even had in 800 ℃, 2 seconds of requirements and extinguish, so just can cross their client 750 ℃ perfectly safe; Based on this reason, we develop the flame-retardant enhanced PBT material that can stablize by extinguishing in 800 ℃, 2 seconds, meet the demand that client is more and more higher.
Summary of the invention
The object of the invention is to the more and more higher situation of requirement of flame-retardant enhanced PBT material being extinguished in 750 ℃, 2 seconds according to existing market, provide a kind of energy stable by the flame-retardant enhanced PBT material extinguishing in 800 ℃, 2 seconds.
Another object of the present invention is to provide the preparation method of above-mentioned flame-retardant enhanced PBT material.
Above-mentioned purpose of the present invention is achieved by the following technical programs:
A kind of high glow-wire ignition temperature flame-retardant enhanced PBT material, by forming according to the component of mass percent meter as follows: PBT resin 40 ~ 50%, bromide fire retardant system 12 ~ 20%, compound flame retardant system 4 ~ 8%, toughner 1 ~ 5%, oxidation inhibitor 0.2 ~ 0.6%, alkali free glass fibre 32 ~ 37% and processing aid 3 ~ 7%; Wherein, described bromide fire retardant system is that auxiliary flame retardant forms by bromine owner fire retardant and antimony; One or more in nitrogenated flame retardant, phosphorus flame retardant, inorganic synergist, tetrafluoroethylene of described compositional flame-retardant system.
As a kind of preferred version, the moisture of described PBT resin is below 0.1%, and reaching this object can be that PBT resin is dried to 3h at 120 ℃.
As a kind of preferred version, described bromine owner fire retardant and antimony are that the mass ratio of auxiliary flame retardant is 3:1; Described bromide fire retardant is the mixture of brominated epoxy resin, three (tribromophenoxy) triazine, brominated Polystyrene, brominated polystyrene brominated polycarbonates; Described antimony is that auxiliary flame retardant is the mixture of antimonous oxide, antimony peroxide, sodium antimonate.
As a kind of preferred version, in described compound flame retardant system, the mass ratio of nitrogenated flame retardant, phosphorus flame retardant, inorganic synergist and tetrafluoroethylene is: 15 ~ 25:15 ~ 25:40 ~ 60:1 ~ 5; Described nitrogenated flame retardant comprises trimeric cyanamide, melamine cyanurate; Described phosphorus flame retardant comprises triphenylphosphate, dihydroxyphenyl propane two (diphenyl phosphoester), Resorcinols (diphenyl phosphoester), Resorcinol-bis-(2.6-xylyl) phosphoric acid ester, zinc borate; Described inorganic synergist comprises nano imvite, wilkinite, mica, kaolin, talcum powder.
The preparation method of the above-mentioned high glow-wire ignition temperature flame-retardant enhanced PBT material of the present invention is after PBT resin, bromide fire retardant system, compound flame retardant system, oxidation inhibitor and processing aid are mixed, when adding twin-screw extrusion machine to melt extrude, at the 5th joint barrel, introducing alkali free glass fibre melt extrudes, the temperature of extruding is 200 ~ 240 ℃, and screw speed is 400rpm; Finally the material of extruding is carried out cooling, air-dry, pelletizing, crosses strong magnetic, packing, obtain high glow-wire ignition temperature flame-retardant enhanced PBT material finished product.
Compared with prior art, the present invention has following beneficial effect:
Flame-retardant enhanced PBT material of the present invention is brought up to 750 ℃ of glowing filaments in the IEC60695 of European Union standard in 800 ℃, 2 seconds and is extinguished, met client to 750 ℃ of demands that glowing filament is more and more higher, possess simultaneously high strength, good toughness, can rapid shaping, high performance-price ratio etc., can meet the requirement of the electric and household electronic products such as vernier switch, connector, fusible cut-out.
Embodiment
Below in conjunction with embodiment, further explain the present invention, but embodiment does not limit in any form to the present invention.
embodiment 1
First the PBT resin of 44.5% weight is dried at 120 ℃ and within 3 hours, control moisture below 0.1%, subsequently with brominated Polystyrene and the 8% sodium antimonate fire retardant of 10% weight, the antimonous oxide of 4% weight and 2% antimony peroxide fire retardant, the toughner of 2.5% weight, primary antioxidant four (β-(3 of 0.2% weight, 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (1010) and 0.2% auxiliary antioxidant three (2, 4-di-tert-butyl-phenyl) phosphorous acid ester (168), other auxiliary agents of 5% weight are mixed and from metering feeding device, are entered twin screw extruder after 2 minutes and plastify by high speed mixer, melting, at twin screw extruder, add the alkali free glass fibre of 30% weight simultaneously, again through extruding, cooling, cross magnetic, be packaged to be product,
embodiment 2
First the PBT resin of 40.2% weight is dried at 120 ℃ and within 3 hours, control moisture below 0.1%, subsequently with brominated Polystyrene and the 6% sodium antimonate fire retardant of 10% weight, the antimonous oxide of 3% heavy amount and 2% antimony peroxide fire retardant, the toughner system of 3% weight, primary antioxidant four (β-(3 of 0.2% weight, 5-di-tert-butyl-hydroxy phenyl) propionic acid) pentaerythritol ester (1010) and 0.2% auxiliary antioxidant three (2, 4-di-tert-butyl-phenyl) phosphorous acid ester (168), other auxiliary agents of 6% weight are mixed and from metering feeding device, are entered twin screw extruder after 2 minutes and plastify by high speed mixer, melting, at twin screw extruder, add the alkali free glass fibre of 35% weight simultaneously, again through extruding, cooling, cross magnetic, be packaged to be product,
Embodiment 1 and 2 preparation method and technique are as follows:
1, raw-material processing and mixing
PBT resin dries 3 hours at 120 ℃, controls moisture below 0.1%;
Major ingredient and bromide fire retardant system, compound flame retardant system, composite toughner, oxidation inhibitor, lubricant etc. are mixed 2 minutes in high speed mixer, make the abundant dispersed with stirring of each component even;
2, melt extrude
The material mixing is added in twin screw extruder, when melt extruding, introduce alkali free glass fibre melt extrude at the 5th joint barrel, melt extrude temperature between 200-240 ℃, screw speed is 400 revs/min;
3, granulation and aftertreatment
The material of extruding is carried out cooling, air-dry, pelletizing, crosses strong magnetic, is packaged to be finished product;
Performance to the flame-retardant enhanced PBT material of embodiment 1 and embodiment 2 gained is as follows
| Test event | Testing standard | Test condition | Embodiment 1 | Embodiment 2 |
| Ash content (%) | GB 9345 | 750 ℃ of calcinations | 34.5 | 40.2 |
| Proportion (g/cm3） | GB 1033 | 23℃ | 1.72 | 1.76 |
| Tensile strength (Mpa) | GB 1040 | 50mm/min | 120.2 | 125.6 |
| Flexural strength (Mpa) | GB 9341 | 2mm/min | 185.2 | 180.6 |
| Modulus in flexure (Mpa) | GB 9341 | 2mm/min | 8522 | 9241 |
| Notched Izod impact strength (KJ/m2） | GB 1843 | 3.2mm, 23℃ | 8.5 | 9.2 |
| Heat-drawn wire (℃) | GB 1634 | 1.8Mpa,6.4mm | 210 | 212 |
| Flame retardant resistance (Class) | UL94 | 0.8mm | V-0 | V-0 |
| Glow wire temperature | IEC60695 | 800℃ | 800 | 800 |
| CTI（V） | GB T4207 | 2.5mm | 300 | 300 |
The above embodiments are preferred embodiments of the present invention, and all changes of having done according to technical solution of the present invention, when the function producing fails to exceed the scope of technical solution of the present invention, all belong to protection scope of the present invention.